UPLC-CAD柱后补偿结合内参法测定三七中的总皂苷  

Determination of total saponins in Panax notoginseng by UPLC-CAD with postcolumn compensation combined with internal reference method

作　　者：陈翠花[1] 朱珂璇 欧阳柳凤 赵玉男[1] 郭盛[2] 

机构地区：[1]南京中医药大学基础医学院,江苏南京210046 [2]南京中医药大学江苏省方剂协同创新重点实验室,江苏南京210046

出　　处：《中成药》2016年第9期1978-1983,共6页Chinese Traditional Patent Medicine

基　　金：南京中医药大学基础医学院青年科技创新基金资助(14JCQN03);国家自然科学基金资助(81303246);江苏省高校"青蓝工程"教师培养计划资助(2012)

摘　　要：目的通过超高效液相色谱-电喷雾检测器（UPLC-CAD）柱后补偿结合内参法同时测定三七Panax notoginseng（Burk.）F.H.Chen中总皂苷的含有量。方法三七70%乙醇提取物的分析采用AcclaimTMRSLC 120 C18色谱柱（150 mm×2.1 mm,2.2μm）;流动相为0.2%甲酸-乙腈,梯度洗脱;柱温30℃;体积流量0.4 mL/min。内参物为人参皂苷Rg1、Re、Rb1、Rd,LC-MS法鉴定各皂苷结构。结果 4个内参物在各自范围内均呈良好的线性关系（r≥0.999 5）,平均回收率94.88%～106.32%,RSD 2.16%～4.74%。LC-MS色谱图中有20个峰,鉴定出10个人参皂苷、2个三七皂苷和绞股蓝皂苷XⅦ。总皂苷平均含有量454.9μg/m L,在0.496 mg/m L供试品溶液中的平均相对含有量91.72%。结论该方法无需校正因子就能分析三七中的总皂苷,可为该植物的质量控制提供参考。AIM To determine the content of total saponins in Panax notoginseng（ Burk.） F. H. Chen by ultra performance liquid chromatography-charged aerosol detection（ UPLC-CAD） with post-column compensation combined with internal reference method. METHODS The analysis of P. notoginseng 70% ethanol extract was performed on AcclaimTMRSLC 120 C18column（ 150 mm × 2. 1 mm,2. 2 μm）,mobile phase was 0. 2% formic acid-acetonitrile in a gradient elution manner,column temperature was maintained at 30 ℃,and flow rate was0. 4 m L / min. The internal reference substances were ginsenoside Rg1,Re,Rb1 and Rd. LC-MS was applied to identifying the structures of various saponins. RESULTS Four internal reference substances showed good linear relationships within their own ranges（ r≥0. 999 5）,whose average recoveries were 94. 88%- 106. 32% with the RSDs of 2. 16%- 4. 74%. There were twenty peaks in the LC-MS chromatogram,ten ginsenosides,two notoginsenosides and gypenoside XⅦ were identified. The average content of total saponins was 454. 9 μg / m L,whose average relative content in 0. 496 mg / m L sample solution was 91. 72%. CONCLUSION This method can analyze the total saponins in P. notoginseng without correction factor,which provides a reference for the quality control of this plant.

关 键 词：三七 总皂苷 UPLC-CAD柱后补偿 内参法 LC-MS 

分 类 号：R284.1[医药卫生—中药学]